#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/85/2018506.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018506
loop_
_publ_author_name
'Duan, Xin-E'
'Tong, Hong-Bo'
'Bai, Sheng-Di'
'Wei, Xue-Hong'
'Liu, Dian-Sheng'
_publ_section_title
;
 meso-Bis{η⁵-1-[1-(dimethylamino)ethenyl]-3-(trimethylsilyl)cyclopentadienyl}iron(II)
 and the cobalt(II) analogue
;
_journal_coeditor_code           SF3173
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m139
_journal_page_last               m142
_journal_paper_doi               10.1107/S0108270112019312
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Co (C12 H20 N Si)2]'
_chemical_formula_moiety         'C24 H40 Co N2 Si2'
_chemical_formula_sum            'C24 H40 Co N2 Si2'
_chemical_formula_weight         471.69
_chemical_melting_point_gt       353
_chemical_melting_point_lt       355
_chemical_name_systematic
;
meso-bis{η⁵-1-[1-(dimethylamino)ethenyl]-3-
(trimethylsilyl)cyclopentadienyl}cobalt(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                105.531(3)
_cell_angle_beta                 111.101(3)
_cell_angle_gamma                102.658(3)
_cell_formula_units_Z            1
_cell_length_a                   7.891(2)
_cell_length_b                   9.363(3)
_cell_length_c                   10.440(3)
_cell_measurement_reflns_used    1963
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.131
_cell_measurement_theta_min      2.256
_cell_volume                     649.2(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3180
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.8029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             253
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0464P)²+0.1772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                2076
_reflns_number_total             2240
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sf3173.cif
_cod_data_source_block           III
_cod_database_code               2018506
_cod_database_fobs_code          2018506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Co Co1 0.5000 0.0000 1.0000 0.02347(15) Uani d S 1 2
N N1 0.2661(3) -0.1351(2) 0.5285(2) 0.0366(5) Uani d . 1 1
Si Si1 0.36534(10) 0.33374(8) 1.14930(7) 0.03285(19) Uani d . 1 1
C C1 0.3288(3) -0.0069(3) 0.7832(2) 0.0272(5) Uani d . 1 1
C C2 0.2594(3) 0.0526(3) 0.8870(3) 0.0283(5) Uani d . 1 1
H H2 0.1366 0.0042 0.8794 0.034 Uiso calc R 1 1
C C3 0.4037(3) 0.1971(3) 1.0053(3) 0.0279(5) Uani d . 1 1
C C4 0.5682(3) 0.2181(3) 0.9774(3) 0.0289(5) Uani d . 1 1
H H4 0.6880 0.3013 1.0376 0.035 Uiso calc R 1 1
C C5 0.5238(3) 0.0931(3) 0.8436(3) 0.0298(5) Uani d . 1 1
H H5 0.6100 0.0796 0.8024 0.036 Uiso calc R 1 1
C C6 0.2186(3) -0.1477(3) 0.6431(3) 0.0297(5) Uani d . 1 1
C C7 0.0921(4) -0.2758(3) 0.6322(3) 0.0408(6) Uani d . 1 1
H H7A 0.0279 -0.3656 0.5432 0.049 Uiso calc R 1 1
H H7B 0.0668 -0.2764 0.7135 0.049 Uiso calc R 1 1
C C8 0.2561(4) 0.0037(4) 0.4914(3) 0.0490(7) Uani d . 1 1
H H8A 0.1232 -0.0153 0.4250 0.074 Uiso calc R 1 1
H H8B 0.3382 0.0234 0.4431 0.074 Uiso calc R 1 1
H H8C 0.3002 0.0951 0.5815 0.074 Uiso calc R 1 1
C C9 0.1853(5) -0.2786(4) 0.3966(3) 0.0575(8) Uani d . 1 1
H H9A 0.2107 -0.3649 0.4252 0.086 Uiso calc R 1 1
H H9B 0.2448 -0.2621 0.3325 0.086 Uiso calc R 1 1
H H9C 0.0463 -0.3045 0.3438 0.086 Uiso calc R 1 1
C C10 0.5746(4) 0.5225(3) 1.2467(3) 0.0538(8) Uani d . 1 1
H H10A 0.6930 0.5022 1.2919 0.081 Uiso calc R 1 1
H H10B 0.5571 0.5945 1.3230 0.081 Uiso calc R 1 1
H H10C 0.5832 0.5697 1.1760 0.081 Uiso calc R 1 1
C C11 0.1368(4) 0.3667(4) 1.0503(3) 0.0546(8) Uani d . 1 1
H H11A 0.1521 0.4163 0.9827 0.082 Uiso calc R 1 1
H H11B 0.1092 0.4350 1.1221 0.082 Uiso calc R 1 1
H H11C 0.0305 0.2659 0.9947 0.082 Uiso calc R 1 1
C C12 0.3350(4) 0.2487(4) 1.2844(3) 0.0495(7) Uani d . 1 1
H H12A 0.2241 0.1508 1.2323 0.074 Uiso calc R 1 1
H H12B 0.3141 0.3233 1.3566 0.074 Uiso calc R 1 1
H H12C 0.4508 0.2276 1.3349 0.074 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 Co1 C2 . 2_657 180.0000(10)
C2 Co1 C5 . . 65.67(9)
C2 Co1 C5 2_657 . 114.33(9)
C2 Co1 C5 . 2_657 114.33(9)
C2 Co1 C5 2_657 2_657 65.67(9)
C5 Co1 C5 . 2_657 180.0000(10)
C2 Co1 C4 . . 65.68(9)
C2 Co1 C4 2_657 . 114.32(9)
C5 Co1 C4 . . 39.89(9)
C5 Co1 C4 2_657 . 140.11(9)
C2 Co1 C4 . 2_657 114.32(9)
C2 Co1 C4 2_657 2_657 65.68(9)
C5 Co1 C4 . 2_657 140.11(9)
C5 Co1 C4 2_657 2_657 39.89(9)
C4 Co1 C4 . 2_657 180.0
C2 Co1 C3 . . 39.80(9)
C2 Co1 C3 2_657 . 140.20(9)
C5 Co1 C3 . . 66.43(9)
C5 Co1 C3 2_657 . 113.57(9)
C4 Co1 C3 . . 39.00(9)
C4 Co1 C3 2_657 . 141.00(9)
C2 Co1 C3 . 2_657 140.20(9)
C2 Co1 C3 2_657 2_657 39.80(9)
C5 Co1 C3 . 2_657 113.57(9)
C5 Co1 C3 2_657 2_657 66.43(9)
C4 Co1 C3 . 2_657 141.00(9)
C4 Co1 C3 2_657 2_657 39.00(9)
C3 Co1 C3 . 2_657 180.0000(10)
C2 Co1 C1 . . 39.19(9)
C2 Co1 C1 2_657 . 140.81(9)
C5 Co1 C1 . . 38.84(9)
C5 Co1 C1 2_657 . 141.16(9)
C4 Co1 C1 . . 65.85(9)
C4 Co1 C1 2_657 . 114.15(9)
C3 Co1 C1 . . 66.39(9)
C3 Co1 C1 2_657 . 113.61(9)
C2 Co1 C1 . 2_657 140.81(9)
C2 Co1 C1 2_657 2_657 39.19(9)
C5 Co1 C1 . 2_657 141.16(9)
C5 Co1 C1 2_657 2_657 38.84(9)
C4 Co1 C1 . 2_657 114.15(9)
C4 Co1 C1 2_657 2_657 65.85(9)
C3 Co1 C1 . 2_657 113.61(9)
C3 Co1 C1 2_657 2_657 66.39(9)
C1 Co1 C1 . 2_657 180.0000(10)
C6 N1 C9 . . 116.3(2)
C6 N1 C8 . . 117.0(2)
C9 N1 C8 . . 111.9(2)
C10 Si1 C12 . . 110.25(15)
C10 Si1 C3 . . 108.65(13)
C12 Si1 C3 . . 112.33(12)
C10 Si1 C11 . . 110.58(15)
C12 Si1 C11 . . 108.16(14)
C3 Si1 C11 . . 106.82(12)
C5 C1 C2 . . 106.0(2)
C5 C1 C6 . . 127.7(2)
C2 C1 C6 . . 126.3(2)
C5 C1 Co1 . . 68.22(12)
C2 C1 Co1 . . 67.81(12)
C6 C1 Co1 . . 127.23(15)
C1 C2 C3 . . 110.5(2)
C1 C2 Co1 . . 73.00(13)
C3 C2 Co1 . . 72.17(12)
C1 C2 H2 . . 124.8
C3 C2 H2 . . 124.8
Co1 C2 H2 . . 121.7
C4 C3 C2 . . 105.2(2)
C4 C3 Si1 . . 128.71(18)
C2 C3 Si1 . . 125.81(17)
C4 C3 Co1 . . 68.73(12)
C2 C3 Co1 . . 68.03(12)
Si1 C3 Co1 . . 132.05(12)
C3 C4 C5 . . 109.4(2)
C3 C4 Co1 . . 72.27(13)
C5 C4 Co1 . . 69.98(13)
C3 C4 H4 . . 125.3
C5 C4 H4 . . 125.3
Co1 C4 H4 . . 124.0
C1 C5 C4 . . 108.7(2)
C1 C5 Co1 . . 72.93(13)
C4 C5 Co1 . . 70.13(13)
C1 C5 H5 . . 125.6
C4 C5 H5 . . 125.6
Co1 C5 H5 . . 122.9
C7 C6 N1 . . 124.3(2)
C7 C6 C1 . . 121.6(2)
N1 C6 C1 . . 114.1(2)
C6 C7 H7A . . 120.0
C6 C7 H7B . . 120.0
H7A C7 H7B . . 120.0
N1 C8 H8A . . 109.5
N1 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
N1 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
N1 C9 H9A . . 109.5
N1 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
N1 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
Si1 C10 H10A . . 109.5
Si1 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
Si1 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
Si1 C11 H11A . . 109.5
Si1 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
Si1 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
Si1 C12 H12A . . 109.5
Si1 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
Si1 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 C2 . 2.084(2)
Co1 C2 2_657 2.084(2)
Co1 C5 . 2.091(2)
Co1 C5 2_657 2.091(2)
Co1 C4 . 2.093(2)
Co1 C4 2_657 2.093(2)
Co1 C3 . 2.140(2)
Co1 C3 2_657 2.140(2)
Co1 C1 . 2.153(2)
Co1 C1 2_657 2.153(2)
N1 C6 . 1.402(3)
N1 C9 . 1.452(3)
N1 C8 . 1.462(3)
Si1 C10 . 1.853(3)
Si1 C12 . 1.855(3)
Si1 C3 . 1.859(2)
Si1 C11 . 1.868(3)
C1 C5 . 1.412(3)
C1 C2 . 1.422(3)
C1 C6 . 1.477(3)
C2 C3 . 1.439(3)
C2 H2 . 0.9400
C3 C4 . 1.414(3)
C4 C5 . 1.427(3)
C4 H4 . 0.9400
C5 H5 . 0.9400
C6 C7 . 1.329(3)
C7 H7A . 0.9400
C7 H7B . 0.9400
C8 H8A . 0.9700
C8 H8B . 0.9700
C8 H8C . 0.9700
C9 H9A . 0.9700
C9 H9B . 0.9700
C9 H9C . 0.9700
C10 H10A . 0.9700
C10 H10B . 0.9700
C10 H10C . 0.9700
C11 H11A . 0.9700
C11 H11B . 0.9700
C11 H11C . 0.9700
C12 H12A . 0.9700
C12 H12B . 0.9700
C12 H12C . 0.9700
